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Advances in Physics Theories and Applications www.iiste.org ISSN 2224-719X (Paper) ISSN 2225-0638 (Online) Vol 9, 2012 1 Synthesis, Characterization, And Antibacterial Activities Of Manganese (II), Cobalt(II), Iron (II), Nickel (II) , zinc (II) And Cadmium(II) Mixed- Ligand Complexes Containing Amino Acid(L-Valine) And Saccharin N.K. Fayad* , Taghreed H. Al-Noor** and F.H Ghanim** * Iraqia University, Baghdad-IRAQ College of Education, chemistry Department, Ibn -AI-Haithem, University of Baghdad- IRAQ * * Corresponding authors e-mail: [email protected] , [email protected] . Abstract A new six mixed ligand complexes of some transition metal ions Manganese (II), Cobalt(II), Iron (II), Nickel (II) , and non transition metal ion zinc (II) And Cadmium(II) with L-valine (Val H ) as a primary ligand and Saccharin (HSac) as a secondary ligands have been prepared. All the prepared complexes have been characterized by molar conductance, magnetic susceptibility infrared, electronic spectral, Elemental microanalysis (C.H.N) and AA . The complexes with the formulas [M(Val) 2 (HSac) 2 ] M= Mn (II) , Fe (II) , Co(II) ,Ni(II), Cu (II),Zn(II) and Cd(II) L- Val H= (C 5 H 11 NO 2 ) , C 7 H 5 NO 3 S The study shows that these complexes have octahedral geometry; The metal complexes have been screened for their in microbiological activities against bacteria. Based on the reported results, it may be concluded that the deprotonated ligand (L-valine) to (valinate ion (Val ) by using (Na OH) coordinated to metal ions as bidentate ligand through the oxygen atom of the carboxylate group( COO ), and the nitrogen atom of the amine group (NH 2 ), where the saccharin (H Sac) coordinated as a monodentate through the nitrogen atom. Keywords: L-Valine , mixed ligand complexes, Saccharin , spectral studies , Antibacterial activities. Introduction 1 The chemical properties and especially the physiological and biochemical activity of saccharin and its compounds have been intensively investigated mainly because of its suspected carcinogenic nature. In particular, since it has been shown that it causes cancer in rats, saccharin joined the list of human potential cancer-causing substances in USA .[1] The structural data for metal saccharinates and metal complexes including saccharin and various coordinated mono- (imidazole, pyridine) or polycyclic N-donor ligands (2,2'-bipyridine,

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Synthesis, Characterization, And Antibacterial Activities Of Manganese

(II), Cobalt(II), Iron (II), Nickel (II) , zinc (II) And Cadmium(II) Mixed-

Ligand Complexes Containing Amino Acid(L-Valine) And Saccharin

N.K. Fayad*

, Taghreed H. Al-Noor** and F.H Ghanim**

* Iraqia University, Baghdad-IRAQ

College of Education, chemistry Department, Ibn -AI-Haithem, University of Baghdad-

IRAQ * *

Corresponding authors e-mail: [email protected] , [email protected] .

Abstract A new six mixed ligand complexes of some transition metal ions Manganese (II),

Cobalt(II), Iron (II), Nickel (II) , and non transition metal ion zinc (II) And

Cadmium(II) with L-valine (Val H ) as a primary ligand and Saccharin (HSac) as

a secondary ligands have been prepared. All the prepared complexes have been

characterized by molar conductance, magnetic susceptibility infrared, electronic

spectral, Elemental microanalysis (C.H.N) and AA . The complexes with the

formulas [M(Val)2(HSac)2]

M= Mn (II) , Fe (II) , Co(II) ,Ni(II), Cu (II),Zn(II) and Cd(II)

L- Val H= (C5H11NO2) , C7H5NO3S

The study shows that these complexes have octahedral geometry; The metal

complexes have been screened for their in microbiological activities against

bacteria. Based on the reported results, it may be concluded that the deprotonated

ligand (L-valine) to (valinate ion (Val) by using (Na OH) coordinated to metal

ions as bidentate ligand through the oxygen atom of the carboxylate group(COO

), and the nitrogen atom of the amine group (NH2), where the saccharin (H Sac)

coordinated as a monodentate through the nitrogen atom.

Keywords: L-Valine , mixed ligand complexes, Saccharin , spectral studies , Antibacterial

activities.

Introduction – 1 The chemical properties and especially the physiological and biochemical activity of

saccharin and its compounds have been intensively investigated mainly because of its suspected

carcinogenic nature. In particular, since it has been shown that it causes cancer in rats, saccharin

joined the list of human potential cancer-causing substances in USA .[1]

The structural data for metal saccharinates and metal complexes including saccharin and

various coordinated mono- (imidazole, pyridine) or polycyclic N-donor ligands (2,2'-bipyridine,

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1,10-phenantroline) were retrieved from the Cambridge Structural Database and analyzed. The

influence of the nature of the metal ion and of the type of the metal-to-ligand bonding on the

saccharinato geometry was examined. The structural data obtained by X-ray diffraction .[2-3]

Studies of mixed ligand complexes containing saccharinate and some other ligands have

demonstrated that the coordination mode of saccharinate is highly adaptable to the steric

requirements of the complex formed. [3-4] The coexistence of bonded and non-bonded

saccharinate anions has also been demonstrated in a number of cases. Also the presence of non-

deprotonated saccharin molecules in a number of complex structures has been established. .[4]

Saccharin is a non nutritive sweetener, meaning that it is not metabolized by the body to

produce energy. [5] Saccharin (C7H5NO3S), also called o-sulfobenzoimide, is widely used as an

artificial sweetening agent. Saccharin is a weak acid [1] .

Figure (1) formulae Saccharin and L-Valine

saccharinate moiety can act either as a single bidentate ligand for only one metal center or,

more frequently, as a bidentate bridging ligand. A recent example for the first situation is the

complex [Pb(sac)2ophen(H2O)2 ] (ophen = 1,10-phenanthroline) in which Pb(II) presents the

unusual coordination number eight, with the two saccharinate anions acting as bidentate and the

coordination sphere completed by the two N atoms of ophen and the two water O-atoms[6] . In

the case of the simpler [Pb(sac)2].H2O complex, the bidentate ligand originates a dimeric

structure. [7]

Besides, the presence of free saccharin in the crystal lattices of certain complexes have been

established, as mentioned above in the case of the [Ln(sac)2(H2O)6](sac)(Hsac).4H 2O complexes

[8] Not withstanding, the first case in which this situation was found is, apparently, the VO2+

complex of composition [VO(OH)(sac) (H2O)2(Hsac)] [4]

L-Valine is essential amino acid [8] widely distributed but rarely occurs in amount exceeding

10%. It is branched chain amino acid and can be derived from alanine by the introduction of two

methyl group present on α-carbon atom. This is glycogenic. On domination, it forms methyl-

malonyl-CoA which can be converted to succinyl -CoA in place of two H atoms of the methyl

group. [9]

NH2

O

HO

O

NH

S

O

O

L-Valine (C5H11NO2) Saccharin (C7H5NO3S)

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The present investigation deals with the preparation, spectroscopic studies of the complexes

obtained during the reaction of saccharin and L-Valine with Manganese (II),Cobalt(II),Iron

(II),Nickel (II),Zinc (II) and Cadmium(II) ions with the aim of investigating the coordination

mode of saccharin and L-Valine in these complexes.

2- Experimental Section: 2-1. Materials: All of the chemical used throughout this investigation were extra pure grade.

Chemicals Saccharin, (L-Valine), and salts were purchased from Merck and BDH were used

without further purification.All the metal ions Mn(II),Co(II),Ni(II), Fe(II), Zn and Cd(II) were of

Analar grade (BDH). They were used in the form of chlorides without further purification.

2-2. Instruments:

I.R spectra were recorded as KBr discs using Fourier Transform Infrared

Spectrophotometer Shimadzu 24FT-I.R8300. Electronic spectra of the prepared complexes were

measured in the region (200- 1100) nm for 10-3

M solutions in DMF at 25ºC using shimadzu-

U.V-160 A Ultra Violet Visible- Spectrophotometer with 1.000 ± 0.001 cm matched quartz cell

.Identify the metal percentage in the complexes by using Shimadzu flame atomic absorption

Model;6809. Electrical conductivity measurements of the complexes were recorded at 25ºC for

10-3

M solutions of the samples in DMF using pw9527 Digital conductivity meter (Philips).

Elemental microanalysis, was carried out using C.H.N elemental analyzer model 5500-Carlo

Erba instrument. Melting points were recorded by using Stuart melting point apparatus.

Chloride ion content were also evolution by (Mohr method), Magnetic susceptibility

measurements were measured using Bruker magnet BM6.

2-3. General synthesis of the mixed ligand metal complexes[11]

A solution of Saccharin (0.366g, 2mmol) in aqueous ethanol (1:1, 10 ml) and solution

of L-valine (0.234, 2 m mol) in aqueous ethanol (1:1,10 ml) containing sodium hydroxide

(0.08, 2mmol) were added simultaneously to a solution of MCl2.nH2O (1 m mol) in

aqueous ethanol (1:1, 10 ml) in the stoichiometric ratio.[2Val:M: 2SacH].(Scheme 1) the

above solution was stirred for 2o minute and allowed to stand for over night .the product

formed was filtered off ,washed with aqueous ethanol (1:1) and dried in air ,and analyzed

employing standard method .

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H2N

CHC

CH

OH

O

H3C

H3C

+ NaOH2 2

H2N

CHC

CH

O- Na+

O

H3C

H3C

1:1(H2O:C2H5OH)

2

H2N

CHC

CH

O- Na+

O

H3C

H3C

2 + 1:1(H2O:C2H5OH)+MCl2

H2N

CHC

CH

O

O

CH3

CH3

H2N

CH

C

CH

O

OCH3

H3C

M

M= Mn(II) Ni(II),Co(II), Fe(II) ,Zn (II) and Cd(II)

O

NH

SO

O

O

NHS

O

O

O

HN

SO

O

Scheme (1): Schematic representation Preparation of the Complexes [M(Val)2(HSac)]

2-4. Antibacterial Activities: [12]

The antibacterial activity of the ligands and there complexs were tested on Gram positive

bacteria, Staphylococcus aureus (+ve), and( Escherichia coli , Salmonella typhi and

Aeruginosa) (-ve). The solvent used was dimethyl form amid(DMF) and sample from 1 to 200

µg/ml were used. Anti bactericidal activities of each compound were evaluated by the well-

diffusion method.1 cm3 of a 24 h broth culture containing 106 CFU/cm

3 was placed in sterile

Petri-dishes. Molten nutrient agar(15 cm3) kept at ca. 45

oC was then poured in the Petri-dishes

and allowed to solidify. Then holes of 6 mm diameter were punched carefully using a sterile cork

borer and these were completely filled with the test solutions. The plates were incubated for 24h

at 37oC.DMF was used as control. The results are shown in Scheme (2).

3- Results and Discussion 3-1. Characterization of Metal Complexes.

Generally, the complexes were prepared by reacting the respective metal chloride with the

ligands using .[2Val:M: 2SacH]mole ratio, i.e. one mole of metal salt : one mole of saccharin

and two moles of sodium valinate.The synthesis of mixed ligand Metal complexes may be

represented as follows:

2Val H +2NaOH→ 2Val- Na

+ + H2O

2Val- Na

+ + HSac + MCl2 → [M(Val)2(HSac)] + 4H2O + NaCl

(where HSac is Sacarine and Val H is amino acid L-valine ).

The formula weights and melting points , are given in (Table I ).Based on the

physicochemical characteristics (Table I), it was found that all the complexes were non-

hygroscopic, stable at room temperature .The solubility of the complexes of ligands was studied

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in various solvents. The complexes are soluble in dimethyl sulfoxide (DMSO) , dimethyl

formamide (DMF) ,ethanol, water while insoluble in common solvents such as benzene, ether,

and chloroform, .The molar conductance values of the complexes in DMF solvent at 10-3

M

concentration are very low ( < 3) signifying their non-electrolytic nature [13]

3-2. Atomic Absorption and chloride ion content :

The atomic absorption measurements (Table-1) for all complexes gave approximated values

for theoretical values. In conclusion, our investigation this suggest that the ligands acid L- valine

and saccharin coordinate with M (II) forming octahedral geometry.

The analytical and physical data (Table 1) and spectral data (Tables 2 and 3) are compatible with

the suggested structures Figure (2).

3-3. The UV-Visible Spectroscopy and Magnetic measurements:

The magnetic moments of the complexes shown in Table (2) were calculated from the

measured magnetic susceptibilities after employing diamagnetic corrections. The electronic

spectral data of the free ligands saccharin, L-valine and their complexes are summarized in Table

-2 together with the proposed assignments and suggested geometries. The results obtained are in

good agreement with other spectra and the literature. [14-16] The UV-Vis spectrum of the ligand

(saccharin) shows peaks at 275 nm, 340 nm assigned to ( – *) and (n – *) electronic

transitions. The spectrum of the free ligand L-valine), exhibits absorption peak at (280

nm)(35714 cm-1

) and an intense peak at 320 nm (3250cm-1),which assigned to (π→ π*), and

(n→ π*) transition respectively [14]

The Zn(II), and Cd(II) complexes did not display any peak in the visible region, no ligand

field absorptions band was observed, therefore the bands appeared in the spectra of two

complex could be attributed to charge transfer transition. in fact this result is a good agreement

with previous work of octahedral geometry. The room temperature μ eff value for the Co( II)

complexes 3.81 B.M. suggest high spin octahedral geometry, which is further supported by the

electronic spectral data .In the Ni( II) complexes. μ eff value at room temperature are in 3.2

B.M. as expected for six coordinated spin free Ni(II) species. While magnetic susceptibility

measurements for Cd(II), and Zn(II) (d10

)(white complexes) showed diamagnetic as expected

from their electronic configuration . [15,16].μeff for Mn2+

(d5) complex was 4.22 B.M within the

expected spin-only values. [17-19]. While magnetic susceptibility measurements for Cd(II), and

Zn(II) (d10

)(white complexes) showed diamagnetic as expected from their electronic

configuration . [15,16]. The Pale Brown complex [Fe (Val)2 (HSac)2] spectrum showed three

absorptions at wave number (36231)cm-1

related charge transfer. The other two absorption at

(25706)cm-1

and (3696)cm-1

were caused by the electronic transitions 6A1g

4T1g(p) and

6A1g

4A1g,

4Eg(D) respectively. [20].

3-4. FT- Infra red spectra The assignment of some of the most characteristic FT-IR band of the complexes are

summarized in (Table -3) together with those of (Sodium valinate ,and saccharin recorded for

comparative purposes and facilitate the spectral analysis.

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The FT- Infra red spectrum of free ligand (L- valin) exhibited a strong band around

(3095) cml that corresponds to the stretching vibration of (N-H) + (O-H), while another

strong absorption band at (1612) cm-1

is appeared which could explained as (- )asy where

the (- ) sym was noticed at (1473) cm-1

.

The Fourier transform infrared spectrum of free ligand saccharin exhibits a weak band at

3095 cm-1

due to the (N-H) vibration [21-22]. The region involving the carbonyl stretching

vibrations is relatively complex, as both the C=O vibrations of saccharin and of the Imine group

lie closely together, and of the NH2 moiety are expected in the same region [23]. The two SO2-

stretching vibrations appear at similar frequencies(1298 and 1163 cm-1

for as(SO2) and s (SO2),

respectively. [21-24].Absorption bands in the (680-636)cm-1

region are considered to be due to

metal-nitrogen vibrations [20-21] whilst those occurring around (536-581)cm-1

are thought to

arise from metal-oxygen vibration . [20-22]

3-5. Proposed molecular structure Studying complexes on bases of the above analysis , the existence of Hexa coordinated

[M(C7H5NO3S)2(C5H11NO2)2] abbreviated as [M(HSac)2(Val)2] were, M(II)=Mn(II),

Ni(II),Co(II), Fe(II),Zn(II) and Cd(II). proposed models of the species were built with chem. 3D

shows in Figure(2).

H2N

CHC

CH

O

O

CH3

CH3

H2N

CH

CCH

O

OCH3H3C

M

O

NHS

O

O

O

HN

SO

O

M= Mn(II) Ni(II),Co(II), Fe(II) ,Zn (II) and Cd(II)

geometrical structure of the complexes-3D Figure (2) : The proposed structure and

3-6. Antibacterial activity

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The antibacterial activity of mixed ligand complexes 1-6 against Staphylococcus aureus

(+ve), and Escherichia coli , Salmonella typhi and Aeruginosa) (-ve) were carried out by

measuring the inhibition diameter .The test compounds were prepared at a concentration of

200 μg / mL. Solvent control that is, DMF was also maintained throughout the experiment

simultaneously .The data are given in Table 4 Scheme (2),It is evident from the above data that

the antibacterial activity significantly increased on coordination. It has been suggested that the

ligands with nitrogen and oxygen donor systems inhibit enzyme activity. Coordination reduces

the polarity of the metal ion mainly because of the partial sharing of its positive charge with the

donor groups within the chelate ring system.(23,24). .Hence produce metal chelates can be

employed as antibacterial.[24]

4- Conclusion: In this paper new mixed ligand complexes containing L-valine and saccharin with the

general formula [M(HSac)2(Val)2] where Synthesis and Characterization of Mixed Ligand

Complexes of L-valine and saccharin with Mn(II), Ni(II), Co(II), Fe(II), Zn(II) and Cd(II) ions .

The molar conductivity of the complexes in DMF solution were non electrolyte. The results

showed that the deprotonated ligand (L-valine) to (valinate ion (Val) by using (Na OH)

coordinated to metal ions as bidentate ligand through the oxygen atom of the carboxyl ate

group(COO), and the nitrogen atom of the amine group (NH2), where the saccharin

coordinated as a monodentate through the nitrogen atom. Therefore, Conclusion Thus the

evidences obtained from IR spectra, electronic spectra and magneto chemical measurements

suggest an octahedral configuration Figure(2).

References 1. Groutas, W.C., Epp, J. B., Venkataraman, R., Kuang, R., Truong, T. M., McClenahan, J.

J., and Prakash, O., (1996) Design, synthesis and in vitro inhibitory activity toward human

leukocyte elastase, Cathepsin G proteinase 3 of saccharine-derived sulfones and congeners.

Biooraganic and Medicinal Chemistry 4,pp 1393-1400.

2. Brien Nabors L. O and Gelardi R. C., (1991), Alternative Sweeteners, 2nd ed., New

York, Marcel Dekker Inc..

3. Enrique J. Baran (2005), The saccharinate anion: a versatile and fascinating ligand in

coordination chemistry , Quím. Nova vol.28 no.2 São Paulo .

4. Ferrer, E. G.; Etcheverry, S. B.; Baran, E. J.(1993); Darstellung und Eigenschaften von

Vanadyl(IV)-Saccharinat , J. Monatsh. Chem. 124, p 355.

5. Williams,P.A.M.; Ferrer, E. G.; Pasquevich, K. A.; Baran, E. J.; Castellano,E.E.;Piro,O. E.

(2000), Characterization of Two New Copper(II) Complexes with Saccharinate and

Benzimidazole as Ligands; J. Chem. Crystallogr. 30, p539.

6. Capita L. F.,Vallvey, Valencia M. C. and Arana Nicola E.s, (2004). Food Additives and

Contaminants, Vol. 21, No. 1, pp. 32–41

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7. Enrique J. Baran, ,Claudia C. Wagner ,Miriam Rossi, Francesco Caruso, (2012). Crystal

Structure and IR Spectrum of Diaqua(o-phenanthroline)bis(saccharinato)lead(II),J, Inorganic

Chemistry and general Chemistry August Volume 638, Issue 10 Pp 1383–1645 .

8. Piro, O. E.; Castellano, E. E.; Baran, E. J.; Z. (2002). Anorg. Crystal Chemistry of the

Saccharinato Complexes of Trivalent Lanthanides and Yttrium Allg. Chem. pp 612–619.

9. Rama Rao A V S S (2002). A text Book of biochemistry 9th ed.

10. Sangar F., Sequencess, Sequences and Sequences Ann. (1988). Rev Biochem 57,;pp1-28.

11. Brugger K. (1973). Coordination Chemistry Experimental Methods. London butter

worth's England.

12. Melnick J. And Delbrgs A, (2007). Medical Microbiology. McGraw Hill-USA.

13. Geary W. J. (1971). The use of conductivity measurements in organic solvents for the

characterization of coordination compounds, Coordination Chemistry Reviews, vol. 7, No. 1,

pp. 81–122.

14. Lever ABP. (1984). “ Inorganic Spectroscopy“;, 2nd (Elsevier Science Publisher,

Amsterdam),

15. Yilmaz Veysel; Yilmaz Fatih; Kazak Canan, (2005). J “Transition Metal hemistry”

Volume 30, Number 1, February, pp. 95-102(8).

16.Shriver D.W., Atkins P.W.(2006)."Inorganic Chemistry" 4th Ed, Freeman, New York.

17. Philip H. Rieger (1994), Electron paramagnetic resonance studies of low-spin d5transition

metal complexes Coordination Chemistry Reviews, Volumes 135–136, pp203-286

18. El-Sonbati A.Z., El-Bindary A.A,. and Mabrouk E.M. (1992). Synthesis and Physico-

chemical Studies on Transition Metal Complexes of Symmetric Bis-Schiff Base Ligands.,J.

Transition Met. Chem., 17,p 63.

19. Muglu H. (2003),Firat University Institute of Science and Technology Ph.D. Thesis,

Elazıg, Turkey.

20.Karipcin,F and Kabalcilar.E(2005),;"Spectroscopic and Thermal Studies on Solid

complexes of 4-(2-pyridylazo) resorcinol with Some Transition Metals"; Acta.Chim.Slov;

Vol.54, pp.242-247.

21.Nakamoto K.,(1996). Infrared spectra of Inorganic and coordination compounds, J.

Wiely and Sons, New York , Ed 4th

.

22. Socrates, G.,(1980), Infrared Characteristic Group Frequencies.1stEd J. Wiely and

Sons, New York, 87.

23.Sarika V., Sarita S. and Poonam R. (2012). Synthesis and spectroscopic studies of mixed

ligand complexes of transition and inner transition metals with a substituted benzimidazole

derivative and RNA bases. J. Chem. Pharmaceut. Res. 4(1): pp 693-699

24.Taghreed H. Al-Noor, Taqi Al- Din Abdul- Hadi and Baha M. Daham. (2012), Synthesis

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June 22, pp22-32.

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Table 1-The physical properties of the Compounds

M.C = Molar Conductivity, Valinato anion = Val- = Valine(C5H10NO2)

- , de = decomposition ,, saccharin =

C7H5NO3S

Analysis Calc.(found)

Cl% M.C Λ µS.cm-1

in DMF

N% H% C% M% Calc.

(found)

Mp °c

(de)

Color

M. wt

Compounds

- 1.34 - - - - 183

Off

White

183.19 saccharin (ligand)

(SacH)

- 1.15 - - - - 244 White 117.15 Valine

Nill 1.43 75.8

( 9.1 )

35.4

) 77 53 )

33514

)

33594)

8.41

( 9.1 )

234de Pale -

yellow

653.58 Mn(Val)2 (SacH)2

Nill 1.28 75..

( 9.2 )

4.62

) 35.7 )

33543

) 33593)

8.53

( 9.3 )

222 de Pale

Brown

654.49 Fe (Val)2 (SacH)2

Nill 1.38 75.8

( 9.1 )

35.4

) 35.4 )

34573

) 33543)

8.96

( 9.6 )

128 de Pale red 657.58 Co (Val)2 (SacH)2

Nill 1.20 75.8

( 9.1 )

35.4

) 35.4 )

3457.

) 33543)

8.93

( 9.6 )

128 de Pale

green

657.34 Ni (Val)2 (SacH)2

Nill 1.36 7533

( 9.3 )

35..

(35.8 )

34531

) 3354.)

9.66

( 10. 2

)

208 de White 664.06 Zn(Val)2 (SacH)2

Nill 1.39 8577

( 8.1 )

358.

2) 35. )

345.3

(34594)

15.81

(16.3 )

230 de White 711.06 Cd(Val)2 (SacH)2

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Table 2- Electronic Spectral data, magnetic moment, of the studied compounds

CT=charge transfer

Probable figure

Assignment

eff

(BM)

- (Cm)

-1

λ nm

compounds

- n*

*

- 21422

36363

340

275

saccharin (ligand)

(SacH)

- n*

*

- 35714

31250

323

280

L- Val H

Octahedral 6A1g →4T1g (G)

CT

5. 04 12224

36231

818

278

Mn(Val)2 (Sac H)2

Octahedral 6A1g

4A1g,

4Eg(D)

6A1g

4T1g(p)

CT

5.18 23696

25706

36231

422

389

276

Fe (Val)2 (Sac H)2

Distorted

Octahedral

4T1g

4T1g (p)

4 T1g

4 A2g

CT

3.81

14771

18903

35971

677

529

278

Co (Val)2 (Sac H)2

Octahedral CT 3A2g (F) →

3T1g (P)

332 36231

23866

276

409

Ni (Val)2 (Sac H)2

Octahedral CT 0.0 36231 276 Zn(Val)2 (Sac H)2

Octahedral CT 0.0 36231 276 Cd (Val)2 (SacH)2

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Advances in Physics Theories and Applications www.iiste.org

ISSN 2224-719X (Paper) ISSN 2225-0638 (Online)

Vol 9, 2012

11

Table (3): FT-IR spectral data of mixed ligand complexes of composition [M(Val)2 (SacH

)2

S= sharp, v s= very sharp, w= weak, b= broad, vb = very broad

M – O

M - N (-COO)sym (-COO )asy

(CNS)

asy

asy (SO2)

sym (SO2)

(C - H)alph

(C - H) cy

(N-H)asy

(N-H)sym

Compounds

- - 1473 s 1612 vs - - 2978s 3223 Val –H

- - - - 974m

1298 vs

1178 vs

-

2976v s- sh

3095s

Sac H

540m 667m

1473s

1396vs

1612vs

1570s 918m

1256 m

1151 s

2943s 3140s

Mn(Val)2 (Sac H)2

542m 667m

1425s-

1396vs

1612m-

1587s 918m

1298 m

1166m

2776m 3394m

Fe (Val)2 (Sac H)2

536m 673m 1356vs 1622vs

1583vs 956s;

1290vs

1155 s 2949s

3508-3101

vs

Co (Val)2 (Sac H)2

543m 680m 1352s

1622vs

1581vs

948m

1288 m

1155m

3115m 3336vs

Ni (Val)2 (Sac H)2

581m 648m 1338s

1616vs

1577vs

923 sh

m

1292 m

1147s

2926vs- sh

3441m

3290vs

Zn(Val)2 (Sac H)2

553s m636 1330 m

s2621

m2881 956m

1271 m

2978 s sh

3482

300vs1

Cd (Val)2 (Sac H)2

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Advances in Physics Theories and Applications www.iiste.org

ISSN 2224-719X (Paper) ISSN 2225-0638 (Online)

Vol 9, 2012

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Table 4. Antimicrobial activity of the ligands and metal complexes Against

(Staphylococcus aureus (+ve) and (Escherichia coli, Aeruginosa, Salmonella typhi and

uginosa) (-ve)

Inhibition Zone (mm)

Complexes

Staphylococcu

s aureus

(+ve)

Aeruginosa

(-ve)

Escherichia

coli

(-ve)

Salmonella

typhi

(-ve)

1 6 8 1 DMF

23 6 6 2 (SacH)

23 6 6 2 L-Val H

28 26 22 1 Mn(Val)2 (Sac H)2

28 26 22 8 Fe (Val)2 (Sac H)2

21 26

23 8 Co (Val)2 (Sac H)2

23 26 28 1 Ni (Val)2 (Sac H)2

22 26

23 - Zn(Val)2(Sac H)2

26 21 22 1 Cd (Val)2(Sac H)2

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ISSN 2224-719X (Paper) ISSN 2225-0638 (Online)

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Scheme (2) Inhibitory activity of the ligands and metal complexes Against

(Staphylococcus aureus (+ve) and Escherichia coli, Aeruginosa, Salmonella

typhi and Staphylococcus aureus) (-ve)

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